JPS60149512A - Make-up cosmetic - Google Patents

Abstract

PURPOSE:To provide the titled cosmetic safe to human body, free from irritation to the skin, and having various excellent characteristics, by carrying out the mordant dyeing of fine powder of regenerated fibroin with a specific natural dye using a water-soluble aluminum salt as a mordant, and using the obtained coloring pigment as a colorant. CONSTITUTION:Fine powder of regenerated fibroin having a crystallinity of 10- 35% is subjected to the mordant treatment with an aqueous solution of a mordant comprising a water-sobuble aluminum salt such as aluminum potassium alum, etc., and is dyed with an aqueous solution of a natural dye selected from the pigment of sappanwood, gardenia, saffron, madder, cacao, sumac, cochineal, lac, gromwell, Japanese pagoda-tree, monascus and indigo-plant, or dyed and then treated with mordant to obtain coloring pigment. 1-50wt% pigment is added to a make-up cosmetic based on the whole components to obtain a cosmetic having excellent resistance to light, heat, etc., and giving silky luster and gloss to the skin.

Description

[Detailed Description of the Invention] Zero Hikari is a colorant P (colorant) obtained by mordant dyeing fine powder of recycled fibroin (P + raw silk fibroin) with a specific natural dye using a water-soluble aluminum salt as a mordant. This invention relates to make-up cosmetics that are improved by blending and using. More specifically, it is safe for the human body, has no scum on the skin, has excellent light resistance, heat resistance, bleed resistance, moisture resistance, water resistance, sweat resistance, color tone, adhesion, and extensibility, and leaves a silky luster on the skin. and give a feel-good meeting. This invention relates to improved makeup cosmetics.

Coal tar pigments, which have traditionally been used in makeup, are
Since their toxicity to the human body, such as their pathogenicity and alligenicity, have become a problem, the number of legal color collections that are licensed for use in cosmetics has been decreasing year by year.

A highly safe alternative to coal tar-based dyes (coloring i)
), but natural pigments have poor light resistance and heat resistance, have large hue fluctuations due to P■, and cannot be used in makeup cosmetics because they bleed.

Japanese Patent Publication No. 55-46367 discloses that in order to improve the drawbacks of natural dyes, silk powder (silk powder) was t-immersed in an alkaline aqueous solution in which the natural dye casamine (safflower pigment) was dissolved for dyeing. After that, the cursamine is fixed and insolubilized with an organic acid to form a pigment, and this is blended into an oil-based cream! It is shown.

However, the silk powder that forms the base of this pigment has a high IF rate of 50 to 60%, so it dyes darkly even with cursamine, and cursamine itself has poor light and heat resistance. Not only does it have insufficient properties, but it also has a low affinity with silk, making it difficult to fall off due to friction when applying cosmetics or in the presence of oily substances. This tendency is seen not only with cursamine, but also with other natural pigments as described below.
Even with cloth dyed in deep colors, it was difficult to sufficiently improve light resistance, heat resistance, bleed resistance, color stability, etc.

The inventors of the present invention have carried out intensive research to improve all aspects of conventional technology. Because it is formed by regenerating silk, its form and properties are significantly chemically and physically inconsistent with the starting material silk. It has higher adhesion properties), produces more vivid colors and gives a good tone, and its gloss, feel, and moisturizing properties are also better than those of silk itself.

t2) The specific natural pigments mentioned below that are dyed on regenerated fibroin are well compatible with water-soluble aluminum salts, resulting in chelation and chemical stabilization due to their mordant action (K), as well as better light resistance and heat resistance. properties, bleed resistance, and the ability to impart a colored glaze.

(6) Since the recycled fibroin base material and the pigments that make up Kibori 1's famous color pigments are natural products, the coloring pigments must be harmless and safe to the human body.

(4) Makeup INj containing the bright one-color pigment of the present invention has outstanding light resistance, heat resistance, bleed resistance, moisture retention, elasticity, extensibility, and peritectic T, and has a 74% effect on the skin. −
It is possible to produce a beautiful and stable cosmetic effect (make-up effect) along with the ring's appearance (soft feel, silky touch).

and so on, and completed the present invention.

That is, according to the present invention, using a water-soluble aluminum salt as a mordant, fine powder of regenerated fibroin can be used as Suo pigment, gardenia pigment, saffron pigment, madder pigment, cacao pigment, yellowfin tuna pigment, cochineal pigment, lac pigment, purple root pigment, and kochineal pigment. This makeup cosmetic is colored with an elm pigment obtained by mordant dyeing with a natural pigment selected from the group consisting of , Monanucus pigment, and Ai pigment.

#il the aqueous solution of silk (buoy 10 in), which is what Honkawa Hosoka calls regenerated fibroin! This is fibroin that is regenerated (precipitated) by directing the regenerated fibroin into a fine powder.

The fine powder of regenerated fibroin is, for example, copper-ethylenediamine aqueous solution, copper hydroxide, ammonia aqueous solution, copper hydroxide-alkali-glycerin aqueous solution, lithium bromide aqueous solution,
Silk (fibroin) is dissolved in at least one solvent selected from the group consisting of calcium, magnesium or zinc chloride, Fi nitrate, thymenanate aqueous solution, and sodium thymesyanate aqueous solution, and then dialyzed. Fibroin was prepared by at least one method such as mixing a coagulant salt into an aqueous solution of 5 to 20% by weight of fibroin, blowing air, adjusting the isoelectric point Mf14, ultrasonication, and stirring at a rapid deformation rate. It is obtained by coagulating and precipitating, then dehydrating, drying, and pulverizing.

The crystallinity of regenerated fibroin in fine powder of regenerated fibroin is Fi10-65%, preferably Hl 5-65%.
Get 60%.

In the present invention, natural pigments for dyeing the fine powder of recycled buproin include Suo extract pigment, Suo pigment such as Brasili Z, gardenia extract pigment, gardenia pigment such as crocin, saffron extract pigment, madder extract pigment, and alizarin. Madder pigments such as, cacao extracted pigments, cacao pigments such as bow polyphenol, yellowfin pigments such as berberine, cochineal extracted pigments, cochineal pigments with carmine acid, lac extraction Pigments, thick coloration of laccaic acid, purple root extraction pigment, purple root coloration of shikonin, etc.
Enju extract pigment, Enju pigment such as LV hand, Monascus extract pigment, Monascus pigment such as Monascorubin,
Ai pigments such as ai extract pigments and indigo.

Mordant staining of regenerated fibroin fine powder in the present invention is as follows:
Fine powder of recycled fish loin was mixed with water-soluble aluminum salt (
After mordant treatment by immersing in an aqueous solution of a mordant), dyeing is performed by immersing in an aqueous solution of the natural dye, or after dyeing fine powder of regenerated fibroin with a saliva solution of a natural dye described in IIJ, water-bathable aluminum This is done by immersing it in an aqueous solution (mordant treatment).

Natural color 10n when dyeing regenerated fibroin fine powder
is 0.1 to 5 based on the weight of regenerated fibroin fine powder.
It is within the range of 0 weight 119b. And the dyeing temperature is usually 6
The temperature was 0 to 100°C, and it was dark from 1 to 3 o'clock during dyeing. When mordanting the recycled fine powder of fibroin, the trouble of the water-soluble aluminum bridge (medium! - Qi;) should be within the range of 1 to 1011 tons based on the weight of the recycled fine powder, and The mordanting temperature is 50 to 8°C, and the mordanting time is 1 to 3 hours.

Each aqueous solution**c when dyeing with the above natural dye aqueous solution and mordant treatment with a water-soluble aluminum salt aqueous solution
r) Amount<bath ratio) is the stone amount VC of the regenerated fibroin fine powder.
It is usually 60 to 70 times the amount.

Examples of the water-soluble aluminum salt include aluminum potassium alum, aluminum sodium alum, aluminum ammonium alum, aluminum sulfate, aluminum chloride, and aluminum chloride.

As mentioned above, the colored face of the present invention obtained by mordant dyeing the fine powder of wild fifu 1 fin, the fine powder of regenerated fibroin and the fine powder of silk (silk powder) without mordanting [5
1-Color-enhancing pigments (normal dyeing) also have dyeability, color development, color, light resistance, heat resistance, bleed resistance, water resistance,
Excellent sweat resistance and adhesion to the skin.

The content of the spring pigment in the makeup cosmetic of the present invention is 1 to 50% by weight based on the total navy blue color of the prescription ingredients.
, preferably 5 to 50% by weight.

The makeup P+ of the present invention can be colored to a desired hue by blending the colored pigments, but if necessary, a small amount of colored inorganic pigments or organic pigments can also be blended.

The bases used in the make-up cosmetic composition of the present invention include inorganic MN, body square pigments, oily substances, fragrances, etc. The makeup 7-pack cosmetics of this publication 1 are extremely useful as, for example, makeup, eye shadow, blush, and fanci makeup.

The makeup cosmetics of the present invention are safe for the human body, do not irritate the skin, and have excellent light resistance, heat resistance, bleach resistance, moisture resistance, water resistance, sweat resistance, color axis, adhesion, and spreadability. Gives a silky luster and feel to the skin (silky touch and good moist feeling@), transparency to the length, and can express and impart a cosmetic effect with good makeup retention (make-up ara 1 effect). Its commercial value is extremely high.

The details will be explained below with reference to examples.

Note that % shown in Examples means % by weight or part by weight. In addition, the test methods for light resistance, heat resistance, bleed resistance, and practical tests (sensory tests) of makeup cosmetics are as follows.

(1) Prepare two light resistance test samples Fi, one placed in a sunlight box (glass case) and exposed to sunlight for two weeks, and one placed in a cool, dark place V.
After 2 weeks of storage for 2 to 11 days, the colors of both samples were compared by visual observation, and the light resistance was determined from the degree of color change.

(Two 2J# thermal test samples were prepared, one was stored in a constant temperature bath with internal peat adjusted to 50℃ for 2 months, and the other was stored in a cool dark place (5℃) for 2 months, and after 2 months The colors of both samples were compared by visual observation, and the heat resistance was determined from the degree of color change.

In addition, in the light resistance test (1) above and this heat resistance test, the Hunter colorimetric L weight, a
value and bfjIi using a spectrophotometer (Newly manufactured by Murakami Color Research)
The color difference Δg was calculated from the following formula and displayed.

△E (color difference) = 〆] Gu7roataku ``koX; = 5' ten (△b5
7.When the ΔE value (color difference value) is 5 or less, the colors of both samples appear to be the same to the naked eye and there is no color difference; when the ΔE value (color difference value) is 5 or more and 10 or less, a slight color difference is perceived; and when the ΔE value is 10 or more and 20 or less, there is a color difference #'i. It can be judged with bias. When the ΔE value for the length is 20 or more, there will be an extremely large color difference.

(5) Bleed resistance test 1 ton of sample was placed in 150 cc of Sa ice water and boiled for 2 hours, and the degree of elution of natural pigments into the water layer (the extent to which the water is colored) was observed with the naked eye to determine the bleed resistance. determined the gender.

(4) Practical test (sensory test) Make-up 111: Color tone, gloss, adhesion to skin, water resistance (sweat resistance), moist feeling when using PF sample for 2 months , regarding makeup longevity and skin clarity.
A sensory test (practical test) was conducted by 50 female panelists, and the results were displayed as sensory evaluation scores. The sensory evaluation score is the average of 60 people for each questionnaire item (test item), where those who answered good were given 5 points, those who answered fair were given 3 points, and those who answered poor were given 1 point. It is a point.

Example 1 (1) Manufacture of all (fine powder of madder dye-mordant dyed regenerated fibroin) of wood-based madder i The mixture was filtered to obtain 39.6 t of an achromatic dyeing solution containing ISl and madder pigment (extracted pigment). In this dye solution, 55% of fine powder of regenerated fibroin (crystallinity 60%) is added.
001 was dispersed and dyed at 60 to 100°C for 1 hour, followed by filtration and thorough washing with water to dissolve and remove free madder pigment.

The obtained madder color collection - fine powder of staining diseased fibroin (
5029) was dispersed in an aqueous solution of aluminum potassium alum 10F dissolved in 2.5 t of water.
After mordant treatment by heating at 0° C. for 30 minutes, the mixture was filtered, thoroughly washed with water, and dried to obtain a reddish-orange colored pigment (madder dye-mordanted dyed regenerated fibroin fine powder).

(2) Production of Kibori J lipstick 9 parts candelilla wax, 8 parts solid paraffin, 5 parts beeswax, 5 parts carnauba wax, 11 parts lanolin, 1 part castor
1344.8i and 10.4 parts of isopropyl myristate were mixed and melted by heating to 80°C, and 6.8 parts of fine powder of madder dye-mordant dyed regenerated fibroin was added to this molten mixture and rolled with a roller. After kneading over
It was melted again, poured into a mold, and cooled to obtain the mold of the present invention.

The color difference in light resistance of the obtained lipstick was 6.1, and the color difference in heat resistance was 3.2, so the color difference was small, and the light resistance and heat resistance were good. In addition, the bleed resistance was good with no dye elution. In addition, the color # (color) of this lipstick, adhesion (feel (moist feel, silky feel) on the skin)
The skin clarity #i was extremely good.

Comparative Example 1 In place of the dyed regenerated fibroin fine powder in madder dye medium 51, fine powder of madder dye-dyed ancient fibroin which had not been mordanted in (1) of Example 1 was used. A lipstick was produced in the same manner as in Example 1.

The resulting lipstick had a large color difference #'i2i,i in light resistance and a color difference Fi15.5 in heat resistance, and its light resistance and heat resistance were poor.

The bleed resistance was poor due to the dye being eluted.

Comparative Example Z (1) Manufacture of comparative colored pigment (madder pigment-dyed silk fine powder) Instead of the regenerated fibroin fine powder used in Example 1 (1), silk fine powder (silk powder) ( Crystallinity 5
A fine powder of madder dye-dyed silk was obtained by dyeing in the same manner as in (1) of Example 1 (without mordant treatment) except that 1%) was used.

(2) Manufacture of a comparative lipstick The procedure of Example 1 was repeated except that the madder pigment-vehicle 11 used in Example 1 was used in place of the fine powder of dyed fibroin. A comparative lipstick was produced in the same manner as in 2).The color difference in light fastness in this lipstick was 25.
．． 6. The color difference in heat resistance is 17.5, and the color difference is large.
Light resistance and heat resistance were poor. In addition, the bleed resistance was poor due to the dye being eluted.

Example 2゜(1) Production of the colored pigment of the present invention (Fine Powder of Regenerated Fibroin for Suo Pigment - Mordant Dyeing) One piece of Suo bark was immersed in 10 tons of water, boiled for 2 hours, cooled, and filtered. 9.6 tons of dye liquor containing 9 g of Soho pigment (extracted color J+-) was obtained. Disperse 500 g of fine powder of regenerated fibroin (crystallinity 60%) in this dye liquor, boil for 1 hour v5 and dye L. After cooling, add to 100 d1 of a saturated aqueous solution of aluminum ammonium micoupan,
A dark medium treatment was carried out at ~80°C for 60 minutes, followed by V-filtration and washing with water. After washing with water, add 1DtK water, add 50IIIg of a 5% aqueous solution of aluminum acetate, carry out mordant treatment at 70 to 80°C for 30 minutes, filter, wash with water, dry, and produce a purple-blue colored pigment (Suaro pigment - mordant dyed fibroin). A fine powder was obtained.

(2) Production of lipstick of the present invention The procedure was carried out in the same manner as (2) of Example 1, except that instead of the fine powder of madder pigment-mordant dyed regenerated fibroin, fine powder of Suho pigment-mordant dyed regenerated fibroin was used. We have produced a lipstick with this original product. The resulting lipstick had a light resistance color difference of 3.0 and a heat resistance color difference of 1.5, with little fallout and good light resistance and heat resistance. In addition, the bleed resistance was good with no dye elution. Furthermore, the color tone, adhesion, feel, and translucency of the skin of this lipstick were very good.

Comparative Example 6゜Fine powder of Suho dye-dyed surviving fibroin obtained by dyeing in the same manner as in Example 2 (1) except that no mordant treatment was carried out was mixed with madder dye of Fruiting Example 1 (2). A lipstick was similarly produced using the mordant dyed regenerated fibroin in place of the fine powder. Color difference in light resistance of the obtained lipstick tf20.1
．． The color difference in heat resistance was 15.5, which was large, and the light resistance and heat resistance were poor. In addition, the bleed resistance was poor due to the dye being eluted.

Example 3゜(1) f! J Zou Shikon 1 kg crushed and soaked in 1 ton of water, 40 ~
Add water 201 at 60℃ and perform dye extraction by hand kneading method to obtain a dye solution containing purple root color #11V.
,9 was obtained. Basic fibroin (crystallinity 30%) is in this dye solution! 50 of'i minutes, 40~60℃ for 2 hours (Haj dyed, purple root dye obtained by dyeing - multiplicative color reproduction) 410 in fine powder 1 to 0.5 f7 Aluminum acetate Dispersed in 20 t of aqueous solution and incubated at 70-60°C for 1 hour.

Mordant treatment was carried out under stirring, washed with water, and dried to obtain a fine powder of regenerated fibroin dyed with purple root dye-mordant.

(2) Production of lipstick of the present invention Same as Example 1 (2) except that a fine powder of purple root pigment-mordant dyed endogenous fibroin is used in place of the fine powder of madder pigment-mordant dyed regenerated fin-loin. A lipstick of the present invention was manufactured by carrying out the following steps. Color difference in lightfastness of the obtained lipstick #
i5.8 and heat resistance color difference 5.1, both of which were small and light resistance and heat resistance were good. In addition, the bleed resistance was good as there was no elution of the dye. 1. This lipstick's color tone, elongation, texture, and skin transparency (feel) were extremely good.

Comparative Example 4゜ Fine powder of purple root dye-dyed regenerated fibroin obtained by dyeing in the same manner as in Example 5 (1) except that the mordant treatment was not carried out was mixed with the madder dye-mordant of (2) in Example WAJ1. A lipstick was produced in the same manner as -1 using the dyed regenerated fibroin fine powder as a substitute.

The obtained comparative lipstick VCh-Lightfastness color difference d30.
5. Color difference in heat resistance H22 and H4 were both large and light resistance and heat resistance were poor. In addition, the bleed resistance was poor due to the dye being eluted.

Example 4゜(1) Colored pigment of the present invention (cochineal color collection medium g/,
Production of (fine powder of dyed regenerated fibroin) Cochineal dye carminic acid ID0fk20t is dissolved in water, and 3296 acetic acid aqueous solution is dispersed in this aqueous solution.
1.5 costo-directional staining at 80'C. After that, aluminum potassium alum 5 f y50- was dissolved in water h
In addition, the same mordanting treatment was carried out by 6 Ω with BO"C.
A fine powder of regenerated fibroin with a striped color was obtained.

(2) Production of lipstick of the present invention The same as in Example 1 (2) except that fine powder of cochineal color book-mordant dyed regenerated fibroin was used instead of fine powder of madder pigment-mordant dyed regenerated fibroin. The company became fJ and began manufacturing J lipsticks. The color difference in light resistance of the obtained lipstick was 5.5, and the heat resistance pigment i'i was +2.5.
01 was also small and the light resistance and heat resistance were good. In addition, the bleed resistance was good with no dye elution. Moreover, the color tone, adhesion, feel, and skin transparency of this lipstick were extremely R-friendly.

Comparative Example 5 +11<! of Example 4 except that no mordant treatment was performed. - A lipstick was produced in the same manner by using the fine powder of cochineal dye-dyed regenerated fibroin obtained by dyeing in the same manner in place of the fine powder of madder dye-mordant dyed regenerated fibroin in (2) of Example 1. did. The color difference 2Z3 in light resistance and the color difference in heat resistance were 15.2, both of which were large compared to the comparison lipsticks obtained, and the light resistance and heat resistance were poor and disappointing. In addition, the bleed resistance was poor due to the dye being eluted.

Example 5゜(1) Production of the colored pigment of the present invention (lac pigment - fine powder of mordant dyed regenerated fibroin) The procedure of Example 4 was repeated except that the lac pigment, laccaic acid, was used in place of the cochineal pigment, carminic acid. Similar to (1), medium gI! Staining was carried out to obtain a fine powder of reddish brown lac dye-mordant dyed regenerated fibroin.

(2) Production of tJJ lipstick from scratch Same as Example 1 (2) except that fine powder of lac dye-mordant dyed regenerated fibroin is used in place of fine powder of madder dye-mordant dyed regenerated fibroin. A lipstick of the present invention was manufactured by carrying out the following steps.

The resulting lipstick had a light resistance color difference of 9.5 and a heat resistance color difference of 3.3, both of which were small, and the light resistance and heat resistance were good. In addition, the bleed resistance was good with no dye elution. In addition, the color tone, adhesion, feel, and skin transparency of this lipstick were excellent among female plants.

Comparative Example 6゜Fine powder of lac dye-dyed regenerated fibroin obtained by dyeing in the same manner as in Example (1) except that no mordant treatment was carried out was mixed with madder dye-vehicle 51 of Example 1 (2). ! ! A lipstick was similarly produced using the dyed regenerated fibroin fine powder as a substitute. The color difference in light resistance of the obtained comparative lipstick was 18.5, and the color difference in heat resistance was 16.7, both of which were large, and the light resistance and heat resistance were poor. In addition, the bleed resistance was poor as color 8iI was eluted.

Example 6゜(1) Production of colored face% of the present invention (monascus dye - fine powder of mordant dyed regenerated fibroin) 150 ft of water-soluble Monascus dye was dissolved in 20 tons of water, and this aqueous solution was added with a VC30% caustic soda aqueous solution to adjust the pH. 11, and this was used as a dye solution. After dispersing 500 g of regenerated fibroin (crystallinity 3 [9b) in this dye solution and dyeing at 60°C for 1 hour, 50% of a 10% aqueous solution of aluminum ammonium alum was added and
A mordant treatment was carried out for a minute. After mordanting, add 4R hydrochloric acid and
The mixture was filtered after adjusting H to 5, washed with water, and dried to obtain a reddish-brown fine powder of Monascus dye-mordant dyeing-regenerated fibroin.

(2) Production of lipstick of Honori J A lipstick of the present invention was obtained in the same manner.

The resulting lipstick had a light resistance color difference of 5.1 and a heat resistance color difference of 1.1, both of which were small, and the light resistance and heat resistance were good. In addition, the bleed resistance was 1 good, with no dye elution. In addition, the color tone, adhesion, feel, and skin transparency of this lipstick were extremely impressive.

Comparative Example 2 No mordant treatment #'i A fine powder of Monascus dye-dyed regenerated fibroin obtained by coloring in the same manner as in Example 6 (1) was mixed with Madder dye of Example 1 (2). -Medium 5
4! ! A lipstick was similarly produced using dyed regenerated fibroin instead of fine powder. Color difference in light resistance of the obtained comparative lipstick #'i20.3. Color difference in ripening resistance #i14.
5, both were large, and the light resistance and heat resistance were poor. In addition, the bleed resistance was poor due to the dye being eluted.

Practical Example B (1) Production of the colored pigment of the present invention (saffron dye - fine powder of mordant dyed regenerated fibroin) 1 k (l) of saffron petals was washed with water, immersed in 401 water, boiled for 1 hour, and filtered. Extracted pigment 220 0.05%
Regenerated) 4 groin (crystallinity 15 tIb
) 500 t'r of dispersion, simultaneous dyeing at 70-80°C, filtration, drying, and pulverization to obtain a fine powder of yellow saffron dye-mordant dyed regenerated fibroin.

(2) Madder pigment medium 51 for producing lipstick of the present invention! ! A lipstick of the present invention was obtained in the same manner as in Example 1 (2), except that fine powder of saffron dye-medium Song-dyed regenerated fibroin was used instead of fine powder of multicolored regenerated fibroin. The resulting lipstick had a light resistance color difference if 9.5 and a heat resistance color difference if 6.1, both of which were small, and the light resistance and heat resistance were good. In addition, the bleed resistance was excellent as there was no bleeding of the dye. In addition, the color^, adhesion, feel, and skin transparency of this lipstick were extremely good.

Comparative Example 8゜ Regenerated fibroin without mordant treatment was used in Example 7 (
The procedure was the same as in Example 1 (2), except that the Sarah 2 dye-dyed regenerated fibroin obtained by staining in the same manner as in 1) was used instead of the fine powder of madder dye-mordanted regenerated fibroin. and produced lipstick. The color difference in light resistance of the obtained comparative lipsticks was 57.5, and the color difference in heat resistance was 22.
5, both were large, and the light resistance and heat resistance were poor. In addition, the bleed resistance was excellent in terms of dye elution.

Fruiting Example 8 (1) Production of the colored pigment of the present invention (fine powder of cacao pigment-mordant dyeing regenerated fibroin) One cacao seed was ground, soaked in 40 tons of water, boiled for 2 hours, and then cooled to form a V. Cocoa Oil Field Pigment 56
511 of 0 obtained 59.6 tons of dye liquor containing 1! Disperse 500f of regenerated fibroin (crystallinity 55%) in the solution, boil for 1 hour to dye, cool, add an aqueous solution in which 1 (l) of aluminum potassium Miratsu bread is dissolved,
Mordant treatment was carried out at 80°C for 50 minutes, followed by filtration, washing with water, and drying to obtain a fine powder of brown cocoa dye-mordanted dyed regenerated fibroin.

(2) Production of lipstick of the present invention Except for using fine powder of cacao dye-mordant dyed regenerated fibroin instead of fine powder of madder dye-mordant dyed regenerated fibroin, (2) of Example 1, l! - In the same manner, a lipstick with non-exploited J was obtained. The resulting lipstick had a light resistance color difference of 5.1 and a heat resistance color difference of 6.0, both of which were small.
Light resistance and heat resistance were excellent. In addition, the bleed resistance was very good in terms of dye elution. In addition, the lipstick's color axis, mattiness, texture, and skin transparency were extremely good.

Comparative Example 9 Same as Example 8 (1) except that mordant treatment was not performed.
The cacao pigment-dyed regenerated fibroin fine powder obtained by C staining was used as a substitute for the madder pigment-mordanted dyed regenerated fibroin fine powder in Example 1 (2), and a lipstick was made in the same way! ! ! I left it behind. The obtained comparative lipstick had a color difference in light resistance (tf) of 15.8 and a color difference in heat resistance (ti) of 10.8, with small scratches and poor light resistance and heat resistance. In addition, the bleed resistance was excellent in terms of dye elution.

Example 9 (1) Production of the coloring pigment of the present invention (fine powder of yellowfin tuna dye-mordant-dyed insect pest fibroin) 1 kq of yellowfin trunk endothelium was cut into small pieces, immersed in 40 tons of water, and boiled for 2 hours. Filtered and yellowfin color chart 21? A dye liquor containing 59.6% was obtained. Disperse autogenous fibroin (61% crystallized) 5002 in this dye solution,
The mixture was incubated at °C for 1 hour, filtered, and washed with water. Next, add 10f of aluminum ammonium alum to 2.51VC of water.
Add the dissolved aqueous solution and mordant for 50 minutes at 70-80℃ 3
! l! The mixture was filtered, washed with water, and dried to obtain a fine powder of yellow yellowfin tuna dye and mordant dyed regenerated light 1-in.

(2) Production of lipstick of the present invention In the same manner as (2) of Example 1, except that fine powder of yellowfin pigment-mordant dyed regenerated fibroin was used instead of fine powder of madder pigment-mordant dyed regenerated fibroin. A lipstick of the present invention was obtained. The resulting lipstick had a light resistance color difference of 3.1 and a heat resistance color difference of 1.5, both of which were small and good in light resistance and heat resistance. -4L Bleed resistance was good with no dye elution. In addition, the color tone, wrapability, feel, and texture of this lipstick on the skin were extremely good.

Comparative Example 10 A fine powder of yellowfin dye-dyed regenerated fibroin obtained by dyeing in the same manner as in Example 9 (1), except that no mordant treatment was performed, was mixed with Madder dye +21 of Example 1- A lipstick was produced in the same manner as in 1 using the mordant vermilion regenerated fibroin fine powder as a substitute. The color difference in light resistance and heat resistance of the comparative lipsticks were 14.4 and 11.5, both of which were large, and the light resistance and heat resistance were poor. In addition, the bleed resistance was good in terms of dye elution and cineration.

Example 1u.

(1) Colored face N of the present invention (Ange dye-mordant dyeing ゛Regenerated fibroin fine powder)! Cut 1 kQ of iI-zo engine pods into small pieces, soak them in 25 tons of water, and boil for 1 hour.
5P filtered and containing 9f of Ange pigment! Liquid 24.
7tm run. To this dye solution, add 0.6% aluminum potassium mi-1 uban aqueous solution #25L in advance at 70 to 80'C for 1 hour.
Regenerated fibroin treated with mountain mordant (crystallinity 25%) 5
00ff Dispersion Sase 70~80'CVci Time dyeing, filtration, washing, drying, yellow amber color-A! - Obtain fine powder of mordant-dyed regenerated fibroin.

('2J Manufacture of lipstick of the present invention In place of the fine powder of madder dye-mordant-dyed regenerated fibroin, use the fine powder of magenta-colored yarn-mordan dyed regenerated fibroin (lltt, (see Example 1) Similar to 2), f
] I got a dud lipstick. This lipstick had a light fastness color difference of 4.6 and a fastness color difference of 5.2 (IF: 2), and the light resistance and heat resistance were good. In addition, the bleed resistance was good with no dye elution. Moreover, the color tone, layering properties, feel, and translucence on the skin of this lipstick were greenish and good.

Comparative Example 11゜Fine powder of the dyed regenerated figroin obtained by turning vermilion in the same manner as in Example 10 (1), except that the mordant treatment was not carried out, was mixed with the madder pigment of Example 1 (2). A lipstick was produced in the same manner using mordant-dyed regenerated fibroin fine powder as a substitute.The resulting comparative lipstick had a light resistance color difference of #'i of 24.5 and a heat resistance color difference of #-t of 21.3. The color was large, and the light resistance and heat resistance were poor.The bleed resistance was poor as there was some elution of the dye.

Example 11゜(1) Production of colored pigment of the present invention (fine pigment of blue dye-mordant dyeing regenerated fibroin powder) 1 kg of the powder was ground, dispersed in 40 tons of water, and mixed with 400 g of a 10% aqueous solution of caustic potash and hydrosulfide. 10 also added 400% of the aqueous solution and stirred, then turned to Ffjh,
A dye liquor 39.41 containing 300v of Ai dye was obtained. Into this dye solution, 500 V of regenerated fibroin (crystallinity 51%), which had been mordanted in advance at 70 to 80°C for 1 hour with 0.1% aqueous solution of aluminum ammonium alum 251, was dispersed, and then at 50 to 70°C for 1 hour. After dyeing, filtering, washing with water, and drying, a fine powder of dark blue slow dye-mordant-dyed viable fibroin was obtained.

(2) Production of lipstick of the present invention In place of the fine powder of madder dye-mordant dyed regenerated figloin, dye-mordant tJ1. g1. A lipstick of the present invention was obtained in the same manner as in Example 1 (2+) except that a fine powder of 10% of color regeneration powder was used. The color difference was 4.6, which was small, and the light resistance and heat resistance were good.The bleed resistance was also good, with no dye elution.Also, the color axis, adhesion, feel, The transparency of the skin was extremely good.

Comparative Example 12 - A fine powder of dyed regenerated fibroin (comparative colored illumination material) obtained by dyeing in the same manner as in Example 11 (1) except that no mordant treatment was carried out was used in Example 1. (21 madder pigment - medium 5I! A lipstick was manufactured by using it as a substitute for the fine powder of dyed regenerated fibroin. The resulting lipstick had a light resistance color difference d1s, a, and a heat resistance color difference H14, 2. □Example 12゜(1) Colored face N of Mokiya town (Gardenia pigment-mordant) Production of dyed regenerated fibroin fine powder) Soak one season of gardenia seeds in 40 tons of water and boil for 1 hour.
111L, filtered and 59.L of dye liquor containing gardenia extracted pigment 580f. 'It was 6t*. In this dye solution, 0
．． 05% & acid ammonium water bath solution 40L at 70-80℃
Media 511! 500f of treated regenerated fibroin fine powder (crystallinity 10%) was dispersed and heated at 70 to 80°C.
After time dyeing, a malic acid aqueous solution was added to adjust P■ to 4, V-filtration and drying were carried out to obtain a fine powder of yellow gardenia dye-mordant dyed regenerated fibroin.

(2) Production of lipstick of the present invention The procedure was carried out in the same manner as in Example 1 (2) except that fine powder of gardenia pigment-mordant dyed regenerated fibroin was used instead of fine powder of madder pigment-mordant dyed regenerated fibroin. I got a lipstick from Kibatsu Ljj. The color difference in light resistance of this lipstick was 7.5, and the color difference in heat resistance was 5.5, both of which were small.The light resistance and heat resistance were good, with a score of 6.0, and the bleed resistance was good with no dye elution. Ta. Moreover, the color tone, adhesion, feel, and skin transparency of this lipstick were extremely good.

Comparative Example 13゜ Fine powder of gardenia pigment-vermilion regenerated fibroin obtained by dyeing in the same manner as in Example 12 (1) except that mordant dyeing was not carried out was dyed with madder pigment-mordant dyeing of Example 1 (21). A comparative lipstick 11[+ was produced using recycled fibroin as a substitute.The color difference in light fastness of the obtained lipstick was 31.
2. The color difference in heat resistance is 21.0, and the color difference is large, and the light resistance is
Heat resistance was poor. In addition, as for the bleed resistance, the elution of the dye was good.

Example 13, fine powder of natural dye-mordant dyed regenerated fibroin produced in Examples 1 to 12 (coloring pigment of the present invention), 15.
After mixing 2 parts with 49.8 parts of Shichisusite, 20 parts of kaolin, and 5 parts of titanium oxide, this was mixed with 4 parts of liquid paraffin,
Each of the present invention is prepared by adding and mixing 1 part of ceresin, 2 parts of lanolin, 4 parts of squalane, and 1 s of stearic acid into a molten mixture, followed by crushing, sieving, and stamping into a mold. I got all the red. Table 1 shows the results of the light resistance (color difference), heat resistance (color difference), and bleed resistance of each of the obtained 11 reds.

1st Table 2 Su Fang 5.34.2 〃 6 Purple root 3.82.8” 4 Cutineal 1.6 1.2 5 Lat Ri 2.81.8 〃 6 Monascus 7.54.8〃 7 v Franc 4.43.4” 8 Kaka, t 3.2! 1.0 /19 Yellowfin 5
．． 6 3.1 tt lo enju 3.8 3.2 1/11 ai
1.8 1.1 〃 12 Gardenia 3.2 2.2,.

As is clear from the results in Table 1, 11 containing Haruirogan N (fine powder of natural dye-mordant dyed regenerated fibroin) of the present invention has good light resistance, heat resistance, and bleed resistance. there were. In addition, each test was excellent in pink color (color tone), adhesion, feel (moist feel), and skin transparency (silk-like luster) 1-1&1.

Comparative Example 14 Comparative Example 1, Comparative Example 5 to Comparative Example 1j were substituted for the fine powder of natural dye-mordant dyed regenerated fibroin used in Example 12.
Natural dye used in - fine powder of dyed viable fibroin (
Comparative samples were produced in the same manner as in Example 12, except that a comparative colored pigment was used. Table 2 shows the results of the light resistance, heat resistance, and bleed resistance of each of the obtained pinks.

Comparative Example 1 in Table 2 Akane 16.5 8.0 Defective (dye eluted) 6 Su Fang 43.0 21.
2 N〃 4〃 Purple Root 21.2 18.5 #〃
5 -I Cutineal 20.6 1!1.6 〃〃
6 〃 Ra ri 18.3 12.4 //〃
7 Monascus 45.2 34.2 1/〃 8
〃 Saffron 21.0 15.6.

〃 9 〃 Ka Kao 18.4 8.6 〃〃10
〃 Yellowfin 19.512.1 〃〃11〃 Engie L29.3 19.8 〃〃 12 〃 Me included 17
．． 5 11.3 〃〃16〃 Gardenia 58.2 1
B, 4 // As is clear from the results in Table 2, the light resistance, heat resistance, and bleeding resistance of #Yoya glue containing the comparative coloring pigment (natural pigment - fine powder of dyed regenerated fibroin) are It was defective.

Example 14゜7 parts of fine powder of cocoa dye-mordanted dyed regenerated fibroin (from Example 8) on the colored pigment of the present invention, 5 parts of fine powder of yellowfin tuna dye-mordant dyed regenerated fibroin (from Example 9) 1 part, gardenia color mordant dyeing 2 parts of recycled fibroin fine powder (from Example 12) were used, and these 30 parts of L mica titanium, 45s of sericite, 6 parts of squalane, 5 parts of lanolin, and 4 parts of myristic acid were added to Example 13. The eye shadow of the present invention was manufactured by mixing, pulverizing, and molding in the same manner as in . Practical test (sensory test) of the obtained eyeshadow
As a result, the sensory evaluation points were 4.5 points for color, 4.8 points for gloss, 4.4 points for skin sensitivity, and 4.4 points for water resistance (sweat resistance).
7 fish, texture (moist feel) 4.5 points, makeup retention 4.4 points, skin transparency E! AJ & 4.2 points, very good and rare.

Comparative Example 15゜In place of the rapid coloring pigment of the present invention, 7 parts of Cacao Color 5 (-Vermillion Paper Fine Powder of Chemical Fibroin (from Comparative Example 9)), Yellowfin Tuna Pigment-Fine Powder of Dyed Regenerated Fibroin (Comparative Example 10) Example 14 except that 2 parts of fine powder of gardenia pigment-striation-restricting fibroin (from Comparative Example 15) was used.
Did you do the same and compare the eye shadows? +1-kI was constructed. Sensory evaluation score of the obtained eye shadow: 1j1: 2.7 points for color tone, 2.2 points for gloss, 1.6 points for adhesion to skin,
Water resistance: 1.2 points, feel: 2.8 points, makeup retention: 1.8 points
On the other hand, Toru IIJ11rB with skin had a score of 1.9, which was relatively poor.

Loss n+i Example 15゜5 parts of fine powder of cutineal dye-mordant dyed regenerated fibroin (from Example 5) as the coloring pigment of the present invention, 5 parts of fine powder of cacao dye-mordant dyed regenerated fibroin (reduced hψ1'')
8), 0.5 parts of fine powder of gardenia dye-mordant dyed regenerated fibroin (from Example 12), and these together with 60 mica, 5 mother titanium, and 56 talc.
s1 5 parts of liquid paraffin and 5 s of olive oil in Example 1
The mixture was mixed in the same manner as in Step 5, pulverized, and subjected to tJ molding to produce the almost red color of the present invention. As a result of the practical test of Haha Beni, the sensory evaluation points were 4.4 points for color tone, 3.8 points for gloss, 4.1 points for skin adhesion, 4.4 points for water resistance, and 4.4 points for feel. is 4.2
The results were extremely good, with 4.7 points for make-up retention and 4.2 points for milk transparency.

6 parts of color-regenerating fibroin fine powder (comparative example 6);
Cocoa pigment - Fine powder of dyed regenerated fibroin (Comparative Example 9
A comparative paste was prepared in the same manner as in Example 15, except that 0.5 m of gardenia pigment-dyed regenerated fibroin fine powder (comparative example 15) was used. Obtained almost red sensory evaluation QFi, color tone is 2.11
2.4 points for gloss, 1.7 points for skin adhesion, and 1 point for water resistance.
．． 1 point for feel, 5.1 point for feel, 1.6 point for make-up retention, and 2.2 point for skin transparency, which was relatively poor.

Example 16 As the coloring pigment of the present invention, 05 parts of fine powder of cacao dye-mordanted dyed regenerated fibroin (from Example 8), fine powder of gardenia dye-mordant dyed regenerated fibroin (Example 12)
(from Example 1) 2 parts, madder dye-mordant dyeing regenerated rye 10 in fine powder (from Example 1) 0. (B was used, and these together with 50.5 parts of sericite, 20 parts of kaolin, and 1 part of oxidized tan
5s, 1 part ceresin, 2 parts lanolin, 4 parts squalane,
Stearic acid 1st - Mixed in the same manner as in Example 15, crushed and molded to produce the foundation of the present invention.

As a result of the practical test of the obtained foundation, adhesion was 4.7 points, water resistance was 4.2 points, feel was 4.1 points, makeup durability was 4.1 points, and skin transparency was 4.7 points. In this respect, it was extremely good.

Comparative Example 1 In addition to the colored pigment of the present invention, 0.5 part of cacao pigment-dyed regenerated fibroin fine powder (comparative example 9) and gardenia pigment-dyed regenerated fibroin fine powder (comparative example 15) were added. Example 1 except that 2 parts of ), 0.4 parts of fine powder of madder pigment-dyed regenerated fibroin (from Comparative Example 1) were used.
A comparison foundation was produced in the same manner as in Example 6. The sensory evaluation scores of the obtained foundation were: 1.8 points for color tone, 2.8 points for gloss, 2.4 points for skin adhesion,
Water resistance: 1.4 points, feel: 3.3 points, makeup durability: 1.8 points
The skin clarity was relatively poor with a score of 2.1.

Example 17 As the coloring material III of the present invention, 2 fine powders of purple root dye-mordant dyed regenerated fibroin (from Example 3) and 4 fine powders of cutineal dye-mordant dyed regenerated fibroin (from Example 4) were used. 0.8 parts of saffron dye-mordant dyed viable fibroin fine powder (from Example 7),
These and 20 99. i! Example 1 (2
) was mixed in the same manner as above to produce a lipstick of the present invention. As a result of the practical test of the obtained lipstick, the sensory evaluation score was 4.
5 points, gloss 3.9 points, adhesion to skin 4.4 points, water resistance 4.3 points, feel 4.3 points, makeup durability 4.0 points,
The skin clarity was 4.1 points, which was extremely good.

Comparative Example 18 In addition to the colored pigment of the present invention, 0.3 parts of purple root pigment-dyed regenerated fibroin fine powder (comparative example 4) and cutineal pigment-dyed regenerated fibroin fine powder (comparative example 5) were added. ), 0.8 parts of saffron pigment-stripe color regenerated fibroin fine powder (from Comparative Example 8), except that Example 1 was used.
A comparative lipstick was produced in the same manner as in Example 7. The obtained lipstick had a sensory evaluation score of 2.2 points for color tone, 2.1 points for gloss,
Skin resistance: 3.2 points, water resistance: 1.4 points, feel: 6 points
．． It was relatively poor, with a score of 5 points, 1.6 points for makeup retention, and 1.9 points for skin transparency.

Example 18゜ As a spring-colored complexion of the present invention, cacao pigment medium tJ, 5.0 parts of dyed regenerated fibroin fine powder (from Example 8),
Madder dye-mordant dyeing Regenerated fibroin fine powder (from Example 1) 5.0 parts, yellowfin dye-vehicle 51! ! 5.0 ml of dyed regenerated fibroin fine powder (from Example 9) was used and mixed. This mixture contains 0.9 l-jetanolamine and 0.1 sodium cetyl sulfate.
The mixture was added to an aqueous solution consisting of 48 parts of water and stirred to uniformly disperse it. This dispersion was mixed with 1.5 parts of semenol and
The 7 ante"- I got John Cream.The result of the practical test of this foundation cream,
Sensory evaluation points are 4.5 points for color tone, 6.5 points for gloss, 4.1 points for skin adhesion, 4.6 points for water resistance, 4.5 points for feel, and 4.6 points for makeup durability. The skin translucent LtlI feeling was 4.2 points, which was extremely good.

Comparative Example 19゜In place of the colored pigment of the present invention, 5 parts of cacao pigment-dyed regenerated fibroin fine powder (from Comparative Example 9), 5 parts of madder pigment-dyed regenerated fibroin fine powder (from Comparative Example 1)
A comparative foundation cream was prepared in the same manner as in Example 18, except that 5 parts of yellowfin tuna dye-dyed regenerated fibroin fine powder (comparative example 10) was used.

The obtained foundation cream had a sensory evaluation score of 2.8 for skin tone, 1.6 for gloss, and 6.6 for adhesion to skin.
1.5 points for water resistance, 6.1 points for feel, and 1 point for makeup durability.
．． The score was 5 points, and the skin clarity was 2.1 points, which was relatively poor.

Applicant: Dunobo Co., Ltd.

Claims (1)

[Scope of Claims] (1) Using water-soluble aluminum salt as a medium and dye, fine powder of regenerated fibroin can be used as suo pigment, gardenia pigment, saffron pigment, madder pigment, cacao pigment, yellowfin pigment, yellowfin pigment, cochineal pigment, and lac. Pigments, purple root pigments, engineering color collections,
A make-up cosmetic colored with a field color rlA material obtained by mordant dyeing with a natural pigment selected from the group consisting of mochi2-cuff pigments and mei pigments. Makeara 1 makeup according to claim (1), wherein the water-soluble aluminum salt according to No. 2111J is aluminum potassium alum, aluminum sodium alum, aluminum ammonium alum, aluminum sulfate, aluminum acetate, aluminum chloride, or a combination thereof. (5) The crystallinity of the regenerated fibroin is 10 to 6.
5% of the makeup according to claim (1). (4) The mordant dyeing is performed by mordanting fine powder of regenerated fibroin with an aqueous solution of water-soluble aluminum salt, and then dyeing with a water condensate of a natural dye. (5) The mordant dyeing is carried out by dyeing fine powder of recycled 7410 in with an aqueous solution of a natural pigment and then mordanting with a water-bathable aluminum plum water solution. Makeup Pr described in 1). (6) The makeup cosmetic according to claim (1), wherein the coloring pigment is blended in an amount of 1 to 5014% based on the total amount of prescription ingredients.